ELECTRONIC SUPPORTING INFORMATION
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1 ELECTRONIC SUPPORTING INFORMATION Supramolecular chains of high nuclearity {Mn III 25} barrel-like single molecule magnets Dimosthenis P. Giannopoulos, a Annaliese Thuijs, b Wolfgang Wernsdorfer, c Melanie Pilkington, a George Christou b and Theocharis C. Stamatatos* a a Department of Chemistry, Brock University, L2S 3A1 St. Catharines, Ontario, Canada. Tel: (+1) ext. 3400; tstamatatos@brocku.ca b Department of Chemistry, University of Florida, Gainesville, Florida , USA. c Institut Néel, CNRS, Nanoscience Department, BP 166, Grenoble Cedex 9, France. 1
2 Experimental Section Syntheses. All manipulations were performed under aerobic conditions using materials as received. The organic ligand mpraoh was synthesized by following the same procedure with that reported previously for the similar ligand praoh 2. 1 Caution! Although no such behavior was observed during the present work, perchlorate and azide salts are potentially explosive; such compounds should be synthesized and used in small quantities, and treated with utmost care at all times. [Mn 25 NaO 20 (OMe) 12 (N 3 ) 12 (mprao) 12 (H 2 O) 2 ] n (1): To a stirred, colorless solution of mpraoh (0.12 g, 1.0 mmol) and NEt 3 (0.14 ml, 1.0 mmol) in MeCN/MeOH (20 ml, 2:1 v/v) were added solid Mn(ClO 4 ) 2 6H 2 O (0.36 g, 1.0 mmol) and NaN 3 (0.07 g, 1.0 mmol). The resulting orange solution was stirred for 6 h, during which time all the solids dissolved and the color of the solution changed to dark brown. The solution was filtered, and the filtrate was layered with Et 2 O (40 ml, 1:1 v/v). After four days, X-ray quality dark-brown plate-like crystals of 1. 8MeOH had appeared and were collected by filtration, washed with cold MeCN (1 x 3 ml) and Et 2 O (2 x 5 ml), and dried in air. The yield was 30 %. Selected IR data (KBr): ν= 3338 (sb), 2078 (m), 2057 (vs), 1600 (m), 1481 (m), 1405 (m), 1307 (m), 1060 (m), 989 (m), 670 (mb), 570 (m). 1 M. M. Hania, Asian J. Chem., 2002, 14,
3 Table S1 Bond Valence Sum (BVS) a,b Calculations for Mn Atoms in Complex 1 Atom Mn II Mn III Mn IV Mn Mn Mn Mn Mn Mn Mn Mn Mn Mn Mn Mn Mn a The underlined value is the one closest to the charge for which it was calculated. The oxidation state is the nearest whole number to the underlined value. b An O BVS in the ~ , ~ , and ~ ranges is indicative of non-, singleand double-protonation, respectively. BVS calculations for selected oxygen atoms in 1 gave values of: for O 2-, for MeO -, and 0.23 for H 2 O. 3
4 18.5 Å Fig. S1 Space-filling representation of the Mn 25 cluster unit of the 1D coordination polymer 1, indicating the length of the molecule. Colour scheme: MnIII blue; O red; N green; C gray Å Fig. S2 Space-filling representation and width of the Mn 25 cluster unit of the 1D coordination polymer 1, viewed approximately along the virtual C 3 axis. 4
5 χ M T (cm 3 mol -1 K) Temperature (K) Fig. S3 χ Μ T vs T plot for complex 1. 5
6 30 χ M 'T (cm 3 mol -1 K) Hz 1000 Hz 500 Hz 250 Hz 50 Hz 25 Hz 10 Hz 5 Hz χ M '' (cm 3 mol -1 ) Temperature (K) Fig. S4 The in-phase (χ Μ ) (as χ Μ T, top) and out-of-phase (χ Μ, bottom) vs T ac susceptibility signals for 1. 6
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